The trinuclear complex, Au(3)(MeN=COMe)(3), which displays a number of remarkable properties including solvoluminescence, has been found to undergo electrochemical oxidation with the deposition of long, thin needles on the electrode surface. The electro-deposition process has been studied by cyclic voltammetry, chronoamperometry, and quartz crystal microbalance techniques. The composition of the electrically conducting needles has been determined to be [Au(3)(MeN=COMe)(3)](ClO(4))(0.34) by two complementary methods. The related complex Au(3)(PhCH(2)N=COMe)(3) underwent oxidation at a significantly more positive potential and did not produce a deposit on the electrode surface.